CN102426869A - Photosensitive silver paste, preparation method thereof and electrodes prepared from paste - Google Patents
Photosensitive silver paste, preparation method thereof and electrodes prepared from paste Download PDFInfo
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- CN102426869A CN102426869A CN2011104572877A CN201110457287A CN102426869A CN 102426869 A CN102426869 A CN 102426869A CN 2011104572877 A CN2011104572877 A CN 2011104572877A CN 201110457287 A CN201110457287 A CN 201110457287A CN 102426869 A CN102426869 A CN 102426869A
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Abstract
The invention discloses photosensitive silver paste, a preparation method thereof and electrodes prepared from the paste. The photosensitive silver paste comprises silver powder, glass powder, an organic binder, photoinitiators, reactive diluents and solvents and further comprises 0.1-1 part of oleic acid and 0.1-1 part of stearic acid based on the parts by weight of the silver powder. According to the invention, the stability and storage time of the photosensitive silver paste are effectively improved by adding the oleic acid and stearic acid into the paste.
Description
Technical field
The invention belongs to the electric slurry field, be specifically related to a kind of photosensitive silver paste, preparation method and by its electrode that makes.
Background technology
In recent years, flat panel display reached its maturity.Plasma flat-panel display has occupied consequence owing to have high brightness, high-contrast, low cost and be easy to large scaleization in the large-sized monitor field.Plasma display mainly is made up of prebasal plate and these two glass substrates of metacoxal plate; Prebasal plate is provided with transparency electrode (ITO electrode); On the ITO electrode, be provided with the bus electrode that is used to increase conductivity; Metacoxal plate is provided with addressing electrode and barrier, in each the grid-like display unit that is formed by barrier and addressing electrode, is provided with the red, green, blue three-color phosphor, in the middle of front-back baseboard, is filled with inert gas.When display was worked, the addressing electrode on the metacoxal plate was confirmed luminescence unit, ITO electrode discharge ionized gas, thus excite the light-emitting phosphor in the metacoxal plate barrier.
Existing plasma flat-panel display also needs further to improve aspect image quality and resolution, in order to improve image quality, improves resolution; An extremely important method is exactly the quantity that increases discharge cell; This just means, for the display floater of same size, needs to make more sparking electrode; Therefore, just need the making of electrode meticulousr.More existing plasma display with low resolution and image quality of difference generally all is the electrode that adopts print process to make; The advantage of this method is to save raw material; Weak point is to form high-precision electrode pattern, and along with the increase of print pass, silk screen is easy to generate inelastic deformation; Cause electrode pattern not reach required precision, so people's sight has been transferred on the photoetch method.
Photoetch method also is the electrode method comparatively commonly used of making at present, and this technology is on whole glass substrate, to apply the photoactive electrode slurry, after the drying, hides with mask plate, is ultraviolet ray exposure and the formation sub-image down of 365nm at wavelength.Develop with dilute alkaline soln then, remove the part that does not have exposure, carry out sintering at last at a certain temperature, the electrode pattern that final formation can be conducted electricity.The photoactive electrode slurry of using in this manufacture method; What play electric action mainly is silver powder, and silver powder is bigger with respect to its density of organic carrier, in storage process; Silver powder in the slurry is prone to deposit; Thereby the generation layering causes the stable inadequately and storage time weak point of slurry, thereby can't use.
Summary of the invention
The present invention aims to provide a kind of photosensitive silver paste, the preparation method reaches by its electrode that makes, to solve the technical problem that photosensitive silver paste of the prior art is unstable, the storage time is short.
To achieve these goals; According to an aspect of the present invention; A kind of photosensitive silver paste is provided; Comprise silver powder, glass dust, organic binder bond, light trigger, reactive diluent and solvent, the parts by weight calculating according to silver powder further comprises the oleic acid of 0.1～1 weight portion and the stearic acid of 0.1～1 weight portion.
Further, comprise the silver powder of 20～70 weight portions, the glass dust of 3～10 weight portions, the organic binder bond of 5～20 weight portions, the light trigger of 0.2～3 weight portion, the reactive diluent of 4～20 weight portions, the solvent of 8～30 weight portions.
Further, the particle diameter of silver powder is 0.1～10 μ m.
Further, glass dust is bismuth borosilicate glass frit.
Further, solvent is selected from by BC, acetate of butyl carbitol, gamma-butyrolacton, 2,2,4-trimethyl-1,3-pentanediol mono isobutyrate, N, one or more in the group that N '-dimethyl acetic acid amine, alpha-terpineol are formed.
Further, organic binder bond is the copolymer of methyl methacrylate and methacrylic acid.
Further; Light trigger is selected from by benzophenone, alpha, alpha-dimethyl oxygen base-α-phenyl acetophenone, α; α-diethoxy acetophenone, 2; 4-diethyl-9H-thioxanthene-9-one, 2-hydroxy-2-methyl-1-phenylacetone, 2-phenyl-2-dimethylamino-1-(4-morpholinyl phenyl)-butanone-1,1-hydroxyl-cyclohexyl benzophenone, α-amine alkyl phenones, two benzoyl phenyl phosphine oxide, tetramethyl Michler's keton, 4, one or more in the group that 4 '-two phenoxy group benzophenone are formed.
Further; Reactive diluent is selected from by styrene, butyl acrylate, vinylacetate, 1, and 6-hexylene glycol double methacrylate, two contracts/the two acrylic acid esters, two of tripropylene glycol contract/in the group that the two acrylic acid esters of triethylene Glycol, ethoxyquin bisphenol-A double methacrylate, polyethylene glycol double methacrylate are formed one or more.
According to a further aspect in the invention, above-mentioned each the preparation method of photosensitive silver paste is provided, has comprised the steps: 1) organic binder bond is dissolved in the solvent, stir, obtain solution A; In solution A, add reactive diluent and light trigger, obtain solution B; 2) in solution B, add silver powder, glass dust and account for oleic acid and the stearic acid of 0.1～1 weight portion of 0.1～1 weight portion of silver powder total weight umber while stirring, fully mix, obtain mixture C; 3) with mixture C after three beaming rollers roll, filter, obtain photosensitive silver paste.
In accordance with a further aspect of the present invention, a kind of electrode is provided, this electrode is prepared from above-mentioned each described photosensitive silver paste.
Beneficial effect of the present invention: the present invention is through adding oleic acid and stearic acid, the stability and the storage time of having improved photosensitive silver paste effectively in slurry.
Embodiment
Need to prove that under the situation of not conflicting, embodiment and the characteristic among the embodiment among the application can make up each other.To combine embodiment to specify the present invention below.
According to a kind of exemplary embodiment of the present invention; A kind of photosensitive silver paste is provided; Different with prior art is; Except comprising silver powder, glass dust, organic binder bond, light trigger, reactive diluent and solvent, the parts by weight calculating according to silver powder further comprises the oleic acid of 0.1～1 weight portion and the stearic acid of 0.1～1 weight portion.Adopt technical scheme of the present invention, improved the stability and the storage time of photosensitive silver paste effectively.
In exemplary embodiment of the present invention, this photosensitive silver paste comprises the silver powder of 20～70 weight portions, the glass dust of 3～10 weight portions, the organic binder bond of 5～20 weight portions, the light trigger of 0.2～3 weight portion, the reactive diluent of 4～20 weight portions, the solvent of 8～30 weight portions.The raw material of the photosensitive silver paste of preparation is limited to the system that helps to obtain stable performance in the above-mentioned scope.Wherein, the silver powder of interpolation can be single silver powder, also can be the composition of multiple silver powder, and preferably, the particle diameter of silver powder is 0.1～10 μ m.The particle diameter of the silver powder that adds both can guarantee to form the slurry system of homogeneous in this scope; Help again in the manufacturing process in later stage, can be arranged on more equably on the glass substrate; The photoengraving technology that helps the later stage finally obtains the good electrode of electric conductivity.
The major function of glass dust is that silver powder particles can be bondd and combine closely with substrate behind sintering each other, thereby obtains conductivity and tack preferably.Operable glass dust system is preferably bismuth borosilicate glass frit, plants glass dust but the present invention is not limited thereto.Select for use bismuth borosilicate glass frit more effectively with after silver powder mixes it to be bonded in the substrate.
In another kind of exemplary embodiment of the present invention; The preferred free BC of the solvent of being selected for use, acetate of butyl carbitol, gamma-butyrolacton, 2; 2; 4-trimethyl-1,3-pentanediol mono isobutyrate, N, one or more in the group that N '-dimethyl acetic acid amine, alpha-terpineol are formed.As long as the solvent of being selected for use can make the organic principle dissolving in the system and be inertia to other compositions in the slurry, above-mentioned some organic solvents for using always.
Preferably, organic binder bond is the copolymer of methyl methacrylate and methacrylic acid.Light trigger is selected from by benzophenone, alpha, alpha-dimethyl oxygen base-α-phenyl acetophenone, α; α-diethoxy acetophenone, 2; 4-diethyl-9H-thioxanthene-9-one, 2-hydroxy-2-methyl-1-phenylacetone, 2-phenyl-2-dimethylamino-1-(4-morpholinyl phenyl)-butanone-1,1-hydroxyl-cyclohexyl benzophenone, α-amine alkyl phenones, two benzoyl phenyl phosphine oxide, tetramethyl Michler's keton, 4, one or more in the group that 4 '-two phenoxy group benzophenone are formed.Reactive diluent is selected from by styrene, butyl acrylate, vinylacetate, 1, and 6-hexylene glycol double methacrylate, two contracts/the two acrylic acid esters, two of tripropylene glycol contract/in the group that the two acrylic acid esters of triethylene Glycol, ethoxyquin bisphenol-A double methacrylate, polyethylene glycol double methacrylate are formed one or more.
According to a further aspect in the invention, a kind of preparation method of above-mentioned arbitrary photosensitive silver paste is provided, has comprised the steps: 1) organic binder bond is dissolved in the solvent, stir, obtain solution A; In solution A, add reactive diluent and light trigger, obtain solution B; 2) in solution B, add silver powder, glass dust and account for oleic acid and the stearic acid of 0.1～1 weight portion of 0.1～1 weight portion of silver powder total weight umber while stirring, fully mix, obtain mixture C; 3) with mixture C after three beaming rollers roll, filter, obtain photosensitive silver paste.This preparation method's technology is simple, can be fit to large-scale commercial Application.
In addition, when making, have good levelability and tack, can add certain antifoaming agent and surfactant in order to make this photosensitive silver paste; In order to have excellent storage stability, the ester class of available acidity or alkalescence is regulated the pH value of slurry, and the mostly commercialization of these auxiliary agents no longer specifies at this.
In accordance with a further aspect of the present invention, a kind of electrode is provided, this electrode is prepared from above-mentioned any photosensitive silver paste.
Further specify beneficial effect of the present invention below in conjunction with specific embodiment.
Embodiment 1
1) 5 parts of methyl methacrylates and methacrylic acid copolymer are dissolved in 8 parts of Texanol (2; 2,4-trimethyl-1,3-pentanediol mono isobutyrate; The production of Yi Shi Man) in the solvent; Stir, add afterwards 4 parts of styrene as reactive diluent and 0.2 part of benzophenone as light trigger, obtain solution B;
2) in solution B, add 20 parts of silver powder, 3 parts of bismuth borosilicate glass frits and 0.02 part oleic acid and 0.02 part stearic acid while stirring, wherein bismuth borosilicate glass frit main component is 68wt%Bi
2O
3, 7wt%B
2O
3, 14.5wt%SiO
2, 6wt%Al
2O
3, 4wt%ZnO, 0.5wt%Na
2O fully mixes, and obtains mixture C;
3) with mixture C after three beaming rollers roll, filter, obtain photosensitive silver paste.
Embodiment 2
1) 20 parts of methyl methacrylates and methacrylic acid copolymer are dissolved in 30 parts of BCs, stir, add afterwards 20 parts of vinylacetates as reactive diluent and 3 parts of 2-hydroxy-2-methyl-1-phenylacetones as light trigger, obtain solution B;
2) in solution B, add 70 parts of silver powder, 10 parts of glass dust, and 0.7 part oleic acid and 0.7 part stearic acid while stirring, wherein bismuth borosilicate glass frit main component is 58wt%Bi
2O
3, 10wt%B
2O
3, 18.5wt%SiO
2, 6wt%Al
2O
3, 7wt%ZnO, 0.5wt%Na
2O fully mixes, and obtains mixture C;
3) with mixture C after three beaming rollers roll, filter, obtain photosensitive silver paste.
Embodiment 3
1) copolymer with 12 parts of methyl methacrylates and methacrylic acid is dissolved in 19 parts of solvent alpha-terpineols; Stir; Add 8 part 1 afterwards, 6-hexylene glycol double methacrylate as light trigger, obtains solution B as the two benzoyl phenyl phosphine oxides of reactive diluent and 1.6 parts;
2) in solution B, add 45 parts of silver powder, 6.5 parts of bismuth borosilicate glass frits and account for the oleic acid of 0.25 part of silver powder total weight and 0.25 part stearic acid while stirring, wherein bismuth borosilicate glass frit main component is 60wt%Bi
2O
3, 8wt%B
2O
3, 18.5wt%SiO
2, 6wt%Al
2O
3, 7wt%ZnO, 0.5wt%Na
2O fully mixes, and obtains mixture C;
3) with mixture C after three beaming rollers roll, filter, obtain photosensitive silver paste.
Comparative Examples 1
1) copolymer with 12 parts of methyl methacrylates and methacrylic acid is dissolved in 19 parts of solvent alpha-terpineols; Stir; Add 8 part 1 afterwards, 6-hexylene glycol double methacrylate as light trigger, obtains solution B as the two benzoyl phenyl phosphine oxides of reactive diluent and 1.6 parts;
2) in solution B, add 45 parts of silver powder, 6.5 parts of bismuth borosilicate glass frits while stirring, wherein bismuth borosilicate glass frit main component is 60wt%Bi
2O
3, 8wt%B
2O
3, 18.5wt%SiO
2, 6wt%Al
2O
3, 7wt%ZnO, 0.5wt%Na
2O fully mixes, and obtains mixture C;
3) with mixture C after three beaming rollers roll, filter, obtain photosensitive silver paste.
20 ℃ of held, wherein in good condition is zero with the slurry of the foregoing description 1-3 and Comparative Examples 1, stratified sedimentation or caking take place be cured as *, comparing result is seen table 1.
Table 1
| Project | One week | Three weeks | One month | Two months |
| Embodiment 1 | ○ | ○ | ○ | ○ |
| Embodiment 2 | ○ | ○ | ○ | × |
| Embodiment 3 | ○ | ○ | ○ | ○ |
| Comparative Examples 1 | ○ | ○ | × | × |
Embodiment 1-3 and Comparative Examples 1 from table 1 can find out that the present invention has obtained long photosensitive silver paste stabilization time through in slurry system, adding oleic acid and stearic acid.
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. photosensitive silver paste; Comprise silver powder, glass dust, organic binder bond, light trigger, reactive diluent and solvent; It is characterized in that the parts by weight calculating according to silver powder further comprises the oleic acid of 0.1～1 weight portion and the stearic acid of 0.1～1 weight portion.
2. photosensitive silver paste according to claim 1; It is characterized in that, comprise the silver powder of 20～70 weight portions, the glass dust of 3～10 weight portions, the organic binder bond of 5～20 weight portions, the light trigger of 0.2～3 weight portion, the reactive diluent of 4～20 weight portions, the solvent of 8～30 weight portions.
3. photosensitive silver paste according to claim 1 is characterized in that, the particle diameter of said silver powder is 0.1～10 μ m.
4. according to each described photosensitive silver paste among the claim 1-3, it is characterized in that said glass dust is bismuth borosilicate glass frit.
5. photosensitive silver paste according to claim 4; It is characterized in that; Said solvent is selected from by BC, acetate of butyl carbitol, gamma-butyrolacton, 2,2,4-trimethyl-1; 3-pentanediol mono isobutyrate, N, one or more in the group that N '-dimethyl acetic acid amine, alpha-terpineol are formed.
6. photosensitive silver paste according to claim 4 is characterized in that, said organic binder bond is the copolymer of methyl methacrylate and methacrylic acid.
7. photosensitive silver paste according to claim 4; It is characterized in that; Said light trigger is selected from by benzophenone, alpha, alpha-dimethyl oxygen base-α-phenyl acetophenone, α; α-diethoxy acetophenone, 2; 4-diethyl-9H-thioxanthene-9-one, 2-hydroxy-2-methyl-1-phenylacetone, 2-phenyl-2-dimethylamino-1-(4-morpholinyl phenyl)-butanone-1,1-hydroxyl-cyclohexyl benzophenone, α-amine alkyl phenones, two benzoyl phenyl phosphine oxide, tetramethyl Michler's keton, 4, one or more in the group that 4 '-two phenoxy group benzophenone are formed.
8. photosensitive silver paste according to claim 4; It is characterized in that; Said reactive diluent is selected from by styrene, butyl acrylate, vinylacetate, 1, and 6-hexylene glycol double methacrylate, two contracts/the two acrylic acid esters, two of tripropylene glycol contract/in the group that the two acrylic acid esters of triethylene Glycol, ethoxyquin bisphenol-A double methacrylate, polyethylene glycol double methacrylate are formed one or more.
9. according to the preparation method of each described photosensitive silver paste among the claim 1-8, comprise the steps:
1) organic binder bond is dissolved in the solvent, stirs, obtain solution A; In said solution A, add reactive diluent and light trigger, obtain solution B;
2) in solution B, add silver powder, glass dust and account for oleic acid and the stearic acid of 0.1～1 weight portion of 0.1～1 weight portion of silver powder total weight umber while stirring, fully mix, obtain mixture C;
3) with said mixture C after three beaming rollers roll, filter, obtain photosensitive silver paste.
10. an electrode is characterized in that, said electrode is prepared from each described photosensitive silver paste among the claim 1-8.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106057278A (en) * | 2016-08-05 | 2016-10-26 | 代长华 | Photosensitive electrode slurry and preparation method thereof |
| CN107705877A (en) * | 2017-09-19 | 2018-02-16 | 合肥惠科金扬科技有限公司 | A kind of AMOLED display screens electrode slurry |
| CN111145935A (en) * | 2019-12-16 | 2020-05-12 | 中国人民解放军国防科技大学 | Silver electrode slurry and preparation method and application thereof |
Citations (3)
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|---|---|---|---|---|
| CN101279369A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Method for preparing sheet silver powder with high dispersibility |
| CN101604557A (en) * | 2008-06-11 | 2009-12-16 | 四川虹欧显示器件有限公司 | The plasma display of electrocondution slurry and this slurry of use |
| CN101984494A (en) * | 2010-12-09 | 2011-03-09 | 东南大学 | Anti-settling photosensitive silver paste and preparation method thereof |
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2011
- 2011-12-31 CN CN 201110457287 patent/CN102426869B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279369A (en) * | 2008-05-15 | 2008-10-08 | 金川集团有限公司 | Method for preparing sheet silver powder with high dispersibility |
| CN101604557A (en) * | 2008-06-11 | 2009-12-16 | 四川虹欧显示器件有限公司 | The plasma display of electrocondution slurry and this slurry of use |
| CN101984494A (en) * | 2010-12-09 | 2011-03-09 | 东南大学 | Anti-settling photosensitive silver paste and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106057278A (en) * | 2016-08-05 | 2016-10-26 | 代长华 | Photosensitive electrode slurry and preparation method thereof |
| CN106057278B (en) * | 2016-08-05 | 2017-11-28 | 陆福萍 | A kind of photoactive electrode slurry and preparation method thereof |
| CN107705877A (en) * | 2017-09-19 | 2018-02-16 | 合肥惠科金扬科技有限公司 | A kind of AMOLED display screens electrode slurry |
| CN111145935A (en) * | 2019-12-16 | 2020-05-12 | 中国人民解放军国防科技大学 | Silver electrode slurry and preparation method and application thereof |
| CN111145935B (en) * | 2019-12-16 | 2022-07-15 | 中国人民解放军国防科技大学 | Silver electrode slurry and preparation method and application thereof |
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| CN102426869B (en) | 2013-12-18 |
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